CN109309225B - MoS with strain carbon as carbon source2Preparation method of @ C composite electrode material - Google Patents
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Abstract
The invention provides a MoS using strain carbon as a carbon source2The invention relates to a preparation method of a @ C composite electrode material, in particular to a MoS2The nano flaky MoS is used as a precursor and the corn strain carbon is used as a carbon source, and is subjected to a simple mild hydrothermal method2The carbon material grows on the carbon-based surface of the biomass in situ, and the activated carbon material has large specific surface area and rich pore size structure, MoS2The nano sheet array uniformly grows on the carbon-based surface, the compound shows higher conductivity and a more stable structure due to the synergistic effect, and the electrochemical performance is obviously improved.
Description
Technical Field
The invention relates to the technical field of biomass charcoal material preparation, in particular to MoS using strain charcoal as a carbon source2A preparation method of the @ C composite electrode material.
Background
Under the double pressure of emission reduction and economic development, people tend to be natural, sustainable, abundant and low-cost energy storage materials more and more, and with the increasing increase of sustainable development and environmental friendliness awareness, carbon materials generated by biomass are widely concerned by people in the application of energy storage devices;
the biomass charcoal is a charcoal product obtained by processing various biomass organism materials rich in charcoal, and the biomass charcoal not only has the physicochemical properties of common carbon materials, such as good conductivity, chemical inertness, heat resistance and the like, but also is rich in oxygen-containing functional groups such as hydroxyl, carboxyl and the like, and is more suitable for being used as an electrode material;
transition metal sulfides have received much attention in recent years, among othersRepresentative is two-dimensional layered molybdenum sulfide (MoS)2) The layered transition metal sulfide used as the battery cathode can provide a good diffusion channel for lithium ions, relieve volume expansion of the lithium ions in the process of intercalation-deintercalation, and improve the rate capability and the cycling stability of the battery, and is one of the cathode materials with very good prospect, but the traditional MoS2The nano material has larger volume change in the charge and discharge process, so that the application and development of the nano material in the aspect of energy storage are limited, and the electrochemical performance of the composite of the transition metal sulfide nano material with a two-dimensional structure and the carbon material is obviously improved.
Disclosure of Invention
In order to solve the problems, the invention provides a MoS taking strain carbon as a carbon source2Preparation method of @ C composite electrode material, MoS prepared by using corn strain carbon as carbon source2The application of the @ C composite material as the lithium ion battery negative electrode material shows that the composite material has good cycle stability.
The invention is realized by the following technical scheme:
MoS with strain carbon as carbon source2The preparation method of the @ C composite electrode material comprises the following steps:
step one, preparing strain derived carbon, which comprises the following specific steps:
a. removing impurities from corn kernels, and placing the corn kernels under a humid condition to enable the corn kernels to grow mildewed to obtain mildewed corn strains for later use;
b. cleaning fresh leaves, putting the cleaned fresh leaves into a container, adding hot distilled water into the container to soften the leaves, mashing and grinding the leaves until pasty leaves are obtained, cooling the pasty leaves to room temperature, uniformly coating the pasty leaves on the surface of the mildewed corn strain prepared in the step a, and culturing the mildewed corn strain in a culture medium for 1-3 hours;
c. b, putting the strains cultured in the step b and the culture medium into a tubular furnace, introducing nitrogen as protective gas, and performing carbonization pretreatment to obtain a product A;
d. c, mixing and grinding the product A obtained in the step c and KOH, and putting the mixture into a tubular furnace for activation after uniform grinding to obtain a product B;
e. washing the product B with dilute HCl and distilled water in sequence, correcting the pH to 7.2-7.4, and then putting the product B into an oven for drying to obtain strain derived carbon;
step two, MoS2The preparation method of the @ C composite electrode material comprises the following specific steps:
s1: adding the strain derived carbon obtained in the step one into 30-60 ml of deionized water, adding sodium molybdate and thiourea, and mixing and stirring uniformly to obtain a mixed solution;
s2: carrying out hydrothermal reaction on the mixed solution, and drying for 8-12 h in vacuum to obtain MoS2@ C composite electrode material.
Further, the strain derived carbon is modified strain derived carbon, and the preparation method comprises the following specific steps: the strain derived carbon obtained in the step e is soaked into the strain derived carbon with the concentration of 1 mol.L-1After fully mixing, standing, washing and drying the strain derived carbon, crushing and grinding the dried strain derived carbon to obtain the modified strain derived carbon.
Further, the composition of the culture medium in the step b is g.L-1The glucose-agar gel comprises 30-40% of glucose, 5-15% of peptone and 15-25% of agar.
Further, the temperature of the carbonization pretreatment in the step c is 200-300 ℃, the time is 1-2 h, and the temperature programming rate is 3 ℃ min-1～5℃·min-1。
Further, the ratio of the product A to KOH in the step d is 1: 1-1: 3, the activation temperature in a tubular furnace is 700-900 ℃, and the activation time is 2-3 h.
Further, the concentration of dilute HCl in the step e is 1 mol.L-1。
Further, in the step e, the drying temperature of the oven is 60-80 ℃, and the drying time is 8
h～12h。
Further, the strain in S1 is derived from charcoal and Na2MoO4·2H2O、H2NCSNH2The mass ratio of (A) to (B) is 25-50: 10-20: 18 to 36.
Further, the temperature of hydrothermal reaction in S2 is 160-220 ℃ and the time is 18
h～36h。
The invention has the beneficial effects that:
(1) the invention selects corn strains as the carbon source, has cheap raw materials, wide sources, environmental protection and energy saving, can quickly grow the strain carbon, can obtain a large amount of the strain carbon, and has simple preparation process;
(2) MoS of the invention2The nano-sheet array grows on the carbon-based surface uniformly and forms a core-shell structure, the specific surface area is larger and is 478.27m2·g-1；
(3) MoS prepared by the invention2The @ C composite material has higher specific capacity (714.4mA h g)-1) And has good retention compared to a single material after multiple cycles, showing good and cycle-stable electrochemical performance.
Drawings
FIG. 1 is the MoS prepared in example 12The XRD diffraction pattern of @ C.
FIG. 2 is the MoS prepared in example 12Scanning Electron microscopy of @ C.
FIG. 3 is the MoS prepared in example 12@ C.
FIG. 4 is the MoS prepared in example 12The charge-discharge curves of the @ C electrode material at cycles 1, 2 and 60, respectively.
Detailed Description
The invention will be further illustrated with reference to specific examples:
example 1:
removing impurities from corn kernels, placing the corn kernels under a humid condition to enable the corn kernels to grow mildewed to obtain mildewed corn strains for later use, cleaning 1kg of fresh leaves, placing the cleaned leaves into a container, adding hot distilled water to soften the leaves, mashing and grinding the leaves until pasty leaves are obtained, cooling the leaves to room temperature, uniformly coating the pasty leaves on the surface of the mildewed corn strains, placing the mildewed corn strains in a culture medium for culturing for 1 hour, wherein the culture medium comprises the components in g.L-1Comprises glucose 30, peptone 5 and agar 15, and the cultured strains and the culture medium are placed in a tube after being cultured for 1hIntroducing nitrogen as protective gas into a formula furnace, performing carbonization pretreatment at 300 ℃ to obtain a product A, mixing and grinding the product A and KOH according to the ratio of 1:3, uniformly grinding, and then putting into a tube furnace to activate for 2h at 750 ℃ (filling N into the tube furnace)2Protection, temperature programming 4 ℃ for min-1) Obtaining a product B, and sequentially using the product B with the concentration of 1 mol.L-1Washing the obtained product with dilute HCl and distilled water, correcting the pH value to 7.2-7.4, then drying the product in an oven at 60 ℃ for 12 hours to obtain strain derived carbon, and modifying the strain derived carbon, wherein the preparation method comprises the following specific steps: 1g of strain derived carbon is immersed in 20ml of 1 mol.L-1After fully mixing, standing, washing and drying the strain derived carbon, crushing and grinding the dried strain derived carbon to obtain modified strain derived carbon;
0.5g of the modified strain-derived charcoal and 0.2g of Na were weighed2MoO4·2H2O and 0.36g H2NCSNH2Stirring and dissolving in 60ml deionized water, carrying out hydrothermal reaction for 24h at 210 ℃, and carrying out vacuum drying for 12h at 60 ℃ to obtain the composite material MoS of molybdenum disulfide and strain carbon2@C。
As can be seen from the XRD diffraction pattern of FIG. 1, MoS2The @ C composite material has a sharp diffraction peak and a good crystal form. Diffraction peaks appeared at 13.8 °, 32.8 °, 39.5 ° and 58.3 ° 2 θ, corresponding to MoS, respectively2(002), (100), (103) and (110)
Crystal face (JCPDS card No. 37-1492). A certain degree of broad peak coverage appears between 20 degrees to 30 degrees and 40 degrees to 45 degrees, which corresponds to the (002) and (100) crystal planes of the graphite carbon. It can be seen from fig. 1 that the diffraction peak of the (002) crystal face is relatively obvious, and the diffraction peak of the (100) crystal face is very weak, indicating that the activation of the activating agent on the biochar mainly occurs on the carbon surface with relatively high activity.
As can be seen from the scanning electron micrograph of FIG. 2, the surface C is arrayed with the nano flower ball-shaped MoS2。
As can be seen from the AC impedance graph of FIG. 3, the graph is composed of a semicircle of the high frequency region and a diagonal line of the low frequency region, and the diameter of the semicircle of the high frequency region represents the charge transfer impedance (R)ct) Inclined line of low frequency regionIs Li+Diffusion resistance towards the inside of the electrode material, and MoS is obtained according to the test result2R of @ C compositectAnd 73.8 omega.
MoS according to FIG. 42The MoS can be seen in the charge-discharge curves of the @ C electrode material in cycles 1, 2 and 602The specific first discharge capacity of @ C is 714.4mA h g-1The charging specific capacity is 474.6mA h g -160 th cycle MoS2Specific discharge capacity of @ C of 258.5mA h g-1The charging specific capacity is 255.2mA h g-1Showing MoS after recombination2The @ C electrode material shows good and relatively stable electrochemical performance over multiple cycles.
Example 2:
removing impurities from corn kernels, placing the corn kernels under a humid condition to enable the corn kernels to grow mildewed to obtain mildewed corn strains for later use, cleaning 1kg of fresh leaves, placing the cleaned leaves into a container, adding hot distilled water to soften the leaves, mashing and grinding the leaves until pasty leaves are obtained, cooling the leaves to room temperature, uniformly coating the pasty leaves on the surface of the mildewed corn strains, placing the mildewed corn strains in a culture medium for culturing for 2 hours, wherein the culture medium comprises the components in g.L-1Comprises culturing glucose 35, peptone 20 and agar 20 for 2h, placing the cultured strain and culture medium in a tubular furnace, introducing nitrogen as protective gas, carbonizing at 250 deg.C to obtain product A, mixing product A and KOH at a ratio of 1:2, grinding, and activating at 900 deg.C for 2h (charging N) in the tubular furnace2Protection, temperature programming is carried out at 5 ℃ for min-1) Obtaining a product B, and sequentially using the product B with the concentration of 1 mol.L-1Washing the strain with dilute HCl and distilled water, correcting the pH to 7.2-7.4, and drying the strain in an oven at 80 ℃ for 10 hours to obtain strain derived carbon; modifying strain derived carbon, and specifically comprising the following steps: 1g of strain derived carbon is immersed in 20ml of 1 mol.L-1After fully mixing, standing, washing and drying the strain derived carbon, crushing and grinding the dried strain derived carbon to obtain modified strain derived carbon;
0.5g of the modified strain-derived charcoal and 0.2g of Na were weighed2MoO4·2H2O and 0.36g H2NCSNH2Stirring and dissolving in 60ml deionized water, carrying out hydrothermal reaction for 36h at 220 ℃, and carrying out vacuum drying for 12h at 60 ℃ to obtain the composite material MoS of molybdenum disulfide and strain carbon2@C。
It was subjected to electrochemical performance test, cycle 60 MoS2Specific discharge capacity of @ C is 250.6mA h g-1The charging specific capacity is 245.8mA h g-1。
Example 3:
removing impurities from corn kernels, placing the corn kernels under a humid condition to enable the corn kernels to grow mildewed to obtain mildewed corn strains for later use, cleaning 1kg of fresh leaves, placing the cleaned leaves into a container, adding hot distilled water to soften the leaves, mashing and grinding the leaves until pasty leaves are obtained, cooling the leaves to room temperature, uniformly coating the pasty leaves on the surface of the mildewed corn strains, placing the mildewed corn strains in a culture medium for culturing for 3 hours, wherein the culture medium comprises the components in g.L-1Comprises culturing glucose 40, peptone 15 and agar 25 for 3 hr, placing cultured strain and culture medium in a tubular furnace, introducing nitrogen as protective gas, carbonizing at 200 deg.C to obtain product A, mixing product A and KOH at a ratio of 1:1, grinding, and activating in the tubular furnace at 700 deg.C for 2 hr (charging N)2Protection, temperature programming is carried out at 3 ℃ for min-1) Obtaining a product B, and sequentially using the product B with the concentration of 1 mol.L-1Washing with dilute HCl and distilled water, correcting the pH to 7.2-7.4, and drying in a drying oven at 60 ℃ for 12h to obtain strain derived carbon; modifying strain derived carbon, and specifically comprising the following steps: 1g of strain derived carbon is immersed in 20ml of 1 mol.L-1After fully mixing, standing, washing and drying the strain derived carbon, crushing and grinding the dried strain derived carbon to obtain modified strain derived carbon;
0.25g of modified strain-derived charcoal and 0.1g of Na were weighed2MoO4·2H2O and 0.18g H2NCSNH2Stirring and dissolving in 30ml deionized water, carrying out hydrothermal reaction at 160 ℃ for 18h, and vacuum drying at 60 ℃ for 8h to obtain the composite material of molybdenum disulfide and strain carbonMaterial MoS2@C。
It was subjected to electrochemical performance test, cycle 60 MoS2Specific discharge capacity of @ C is 253.9mA h g-1The charging specific capacity is 249.2mA h g-1。
While there have been shown and described what are at present considered the fundamental principles of the invention, its essential features and advantages, it will be understood by those skilled in the art that the invention is not limited by the embodiments described above, which are merely illustrative of the principles of the invention, but various changes and modifications may be made therein without departing from the spirit and scope of the invention as defined by the appended claims and their equivalents.
Claims (7)
1. MoS with strain carbon as carbon source2The preparation method of the @ C composite electrode material is characterized by comprising the following steps of: the method comprises the following steps:
step one, preparing strain derived carbon, which comprises the following specific steps:
a. removing impurities from corn kernels, and placing the corn kernels under a humid condition to enable the corn kernels to grow mildewed to obtain mildewed corn strains for later use;
b. cleaning fresh leaves, putting the cleaned fresh leaves into a container, adding hot distilled water into the container to soften the leaves, mashing and grinding the leaves until pasty leaves are obtained, cooling the pasty leaves to room temperature, uniformly coating the pasty leaves on the surface of the mildewed corn strain prepared in the step a, and culturing the mildewed corn strain in a culture medium for 1-3 hours;
c. b, putting the strains cultured in the step b and the culture medium into a tubular furnace, introducing nitrogen as protective gas, and performing carbonization pretreatment to obtain a product A; the temperature of the carbonization pretreatment is 200-300 ℃, the time is 1-2 h, and the temperature programming rate is 3 ℃ min-1~5℃·min-1；
d. Mixing and grinding the product A obtained in the step c and KOH, uniformly grinding, and then putting into a tube furnace for activation for 2-3 h to obtain a product B;
e. washing the product B with dilute HCl and distilled water in sequence, correcting the pH to 7.2-7.4, and then putting the product B into an oven for drying to obtain strain derived carbon;
the strain derived carbon is modified strain derived carbon, and the preparation method comprises the following specific steps: the strain derived carbon obtained in the step e is soaked into the strain derived carbon with the concentration of 1 mol.L-1After fully mixing, standing, washing and drying the strain derived carbon, crushing and grinding the dried strain derived carbon to obtain modified strain derived carbon;
step two, MoS2The preparation method of the @ C composite electrode material comprises the following specific steps:
s1: adding the strain derived carbon obtained in the step one into 30-60 ml of deionized water, adding sodium molybdate and thiourea, and mixing and stirring uniformly to obtain a mixed solution;
s2: carrying out hydrothermal reaction on the mixed solution, and drying for 8-12 h in vacuum to obtain MoS2@ C composite electrode material.
2. The MoS using charcoal as carbon source according to claim 12The preparation method of the @ C composite electrode material is characterized by comprising the following steps of: the components of the culture medium in the step b are g.L-1The glucose-agar gel comprises 30-40% of glucose, 5-15% of peptone and 15-25% of agar.
3. The MoS using charcoal as carbon source according to claim 12The preparation method of the @ C composite electrode material is characterized by comprising the following steps of: the ratio of the product A to KOH in the step d is 1: 1-1: 3, and the activation temperature in a tubular furnace is 700-900 ℃.
4. The MoS using charcoal as carbon source according to claim 12The preparation method of the @ C composite electrode material is characterized by comprising the following steps of: the concentration of dilute HCl in step e is 1 mol. L-1。
5. The MoS using charcoal as carbon source according to claim 12The preparation method of the @ C composite electrode material is characterized by comprising the following steps of: and e, drying the oven at the temperature of 60-80 ℃ for 8-12 h.
6. The MoS using charcoal as carbon source according to claim 12The preparation method of the @ C composite electrode material is characterized by comprising the following steps of: s1 strain derived from charcoal and Na2MoO4·2H2O、H2NCSNH2The mass ratio of (A) to (B) is 25-50: 10-20: 18-36.
7. The MoS using charcoal as carbon source according to claim 12The preparation method of the @ C composite electrode material is characterized by comprising the following steps of: the temperature of the hydrothermal reaction in S2 is 160-220 ℃, and the time is 18-36 h.
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